CN110407583B - Method for preparing rare earth silicate ceramic by adopting oxygen-containing precursor chemical vapor deposition - Google Patents

Method for preparing rare earth silicate ceramic by adopting oxygen-containing precursor chemical vapor deposition Download PDF

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CN110407583B
CN110407583B CN201910678637.9A CN201910678637A CN110407583B CN 110407583 B CN110407583 B CN 110407583B CN 201910678637 A CN201910678637 A CN 201910678637A CN 110407583 B CN110407583 B CN 110407583B
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刘永胜
贺芳
董宁
王晶
高雨晴
宋超坤
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Northwestern Polytechnical University
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Abstract

The invention relates to a method for preparing rare earth silicate ceramic by adopting oxygen-containing precursor chemical vapor deposition, which adopts rare earth oxide as a reactant and CH3SiCl3As precursor, CO2And (3) as an oxygen source, hydrogen as a carrier gas and a diluent gas, and argon as a protective gas, and performing chemical vapor deposition to obtain the rare earth silicate ceramic. Can be used for preparing rare earth silicate ceramic powder, can also be used for preparing rare earth silicate ceramic coatings, and rare earth silicate ceramic modified structural ceramics and ceramic matrix composite materials. The preparation temperature of the rare earth silicate ceramic is low, the problem of overhigh preparation temperature of the rare earth silicate ceramic is solved, the preparation process is simple to operate and strong in repeatability, the shape of the material is not affected, the industrial production can be realized, and a new method is provided for preparing the rare earth silicate ceramic and the rare earth silicate modified ceramic matrix composite material by chemical vapor deposition.

Description

Method for preparing rare earth silicate ceramic by adopting oxygen-containing precursor chemical vapor deposition
Technical Field
The invention belongs to the field of preparation process methods of rare earth silicate ceramics, and relates to a method for preparing rare earth silicate ceramics by adopting oxygen-containing precursor chemical vapor deposition.
Background
SiC as a new generation of hot end part material for enginesfthe/SiC material is susceptible to water vapor (H) in a combustion environment at high temperatures2O) corrosion to form volatile products (H)2SiO4Etc.) to seriously affect SiCfService life of the/SiC material. The rare earth silicate has lower volatility, excellent anti-oxyhydrogen corrosion performance, excellent chemical stability and low thermal expansion coefficient in a high-speed gas environment, and can be mixed with SiCfMatching of SiC material. Using rare earth silicates as SiCfThe research on the high-temperature oxidation-resistant coating material of the/SiC material is carried out successively. The reported technologies for preparing yttrium silicate high-temperature oxidation-resistant coating mainly include hot isostatic pressing, slurry coating and sintering, plasma spraying, in-situ formation, hydrothermal electrodeposition, and the like. Most of the preparation processes can prepare ideal coatings only at high temperature. While higher preparation temperature may cause certain damage to the SiC fibers and the matrix, so the development of the low-temperature preparation process is one of the motivation directions of researchers.
Compared with the preparation methods such as a plasma spraying method, slurry dipping and sintering, sputtering, polymer conversion and the like, the chemical vapor deposition method has the following obvious advantages: (1) the preparation temperature is low (about 1000 ℃), and is far lower than the sintering temperature of the traditional ceramics; (2) the gas phase permeability is strong, so that the deposition can be conveniently carried out in the fiber prefabricated body of a large, thin-wall and complex component; (3) by designing reaction raw materials and gases, the deposition preparation of various high-temperature ceramics can be realized.
'A method for preparing coating on rare earth silicate coating and C/SiC composite material surface by Liuyongsheng et al of China northwest industry university' (CN 104356696A) comprises casting slurry of yttrium silicate coating or ytterbium silicate coating on composite material surface, and coating with CH3SiCl3The composite material is used as a precursor, hydrogen is used as carrier gas and diluent gas, the hydrogen is used as protective gas, the flow rate ratio is 1:10:6, the reaction temperature is 1000-1100 ℃, the deposition time is 6-12 hours, the yttrium silicate coating or the ytterbium silicate coating is covered on the surface of the composite material by utilizing chemical vapor reaction, the coating is tightly combined with a substrate, and the coating is dense.
Document 1 "Boakye E E, Keller K A, Mogilevsky P S, Parthasarath T A, Ahrens M A, Hay R S, et al2Si2O7matrix composites[J].Ceramic Engineering&Science proceedings.2013, 33(2):233-2Si2O7) The SiC/SiC composite material as the matrix has more dislocation and fine crack in the rare earth silicate matrix under the action of pressure,the crack deflection is facilitated, and a better bearing effect can be achieved.
Document 2 "Boakye E, Mogilevsky P, Parthasarath T A, Keller K A, Hay R S, Cinibulk M K2Si2O7fiber–matrix interphases for SiC–SiC composites[J]The Journal of the American Ceramic society, 2016,99(2):415-2Si2O7) When the rare earth silicate serving as the SiC/SiC composite material interface is used, the fibers can be obviously pulled out in a fiber push-out and push-in experiment, and the rare earth silicate can be used as the composite material interface.
Therefore, the research on the preparation of the rare earth silicate ceramic by using the chemical vapor deposition has practical significance for improving the ceramic matrix composite.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing rare earth silicate ceramic by adopting oxygen-containing precursor chemical vapor deposition, and rare earth oxide (Re) is added2O3) As reactant, an oxygen-containing gas phase precursor CO is used2The rare earth silicate ceramic is converted into the rare earth silicate ceramic by a chemical vapor deposition process, can be used for preparing rare earth silicate ceramic powder, can also be used for preparing a rare earth silicate ceramic coating, and can be used for preparing rare earth silicate ceramic modified structural ceramic and ceramic matrix composite materials.
Technical scheme
A method for preparing rare earth silicate ceramic by adopting oxygen-containing precursor chemical vapor deposition is characterized by comprising the following steps:
step 1, preparing rare earth oxide slurry: magnetically stirring a solution obtained by mixing water with the weight of 70-80%, polyvinyl alcohol with the weight of 1-2%, ammonium polyacrylate with the weight of 0.5-1% and lithium carbonate with the weight of 1-2%;
adding wt 15-25% of rare earth oxide, and performing ball milling to obtain uniformly mixed semi-compact ceramic matrix composite material impregnated rare earth oxide slurry;
the sum of the weight percentages of the components is 100 percent;
step 2, preparing rare earth silicate by chemical vapor deposition: dipping the semi-compact ceramic matrix composite material in rare earth oxide slurry for 120 ℃; with CH3SiCl3As precursor, CO2As oxygen source, hydrogen gas as carrier gas and diluent gas, argon gas as protective gas, gas flow rate ratio Q (H)2):Q(CH3SiCl3)＝6～9，Q(H2):Q(Ar)＝2～3，Q(H2):Q(CO2) 2-4, wherein the flow of argon is 100-120 ml/min, the pressure in the furnace is kept at 2000Pa, the deposition temperature is 1050-1200 ℃, the heat preservation time is 5-15 h, and the rare earth silicate ceramic is obtained through chemical vapor deposition.
The stirring time in the step 1 is 25-35 min, and the stirring speed is 100-120 r/min.
The rotating speed of the ball milling roller in the step 1 is 120-150 r/min, and the ball milling time is 10-15 h.
The rare earth oxide is yttrium oxide, ytterbium oxide, lutetium oxide and other rare earth oxides.
The particle size of the rare earth oxide is distributed between 0.1 and 20 microns.
Advantageous effects
The invention provides a method for preparing rare earth silicate ceramic by adopting oxygen-containing precursor chemical vapor deposition, which adopts rare earth oxide as a reactant and CH3SiCl3As precursor, CO2And (3) as an oxygen source, hydrogen as a carrier gas and a diluent gas, and argon as a protective gas, and performing chemical vapor deposition to obtain the rare earth silicate ceramic. Can be used for preparing rare earth silicate ceramic powder, can also be used for preparing rare earth silicate ceramic coatings, and rare earth silicate ceramic modified structural ceramics and ceramic matrix composite materials.
The invention firstly proposes that the oxygen-containing gas source is adopted to realize the preparation of the rare earth silicate, provides a new idea for preparing the rare earth silicate by chemical vapor deposition, adopts the chemical vapor deposition in the preparation fields of interfaces, coatings and the like, and is more favorable for realizing the preparation of uniform and compact rare earth silicate layers. Compared with the prior patent, the ceramic matrix composite can be modified at the coating and the base body simultaneously, and more effective is providedThe protective effect of (1). Further, document 3, "Giesche H, Matijevic E.preparation, chromatography, and chromatography of well-defined silicas/ytria powders [ J]The method of beta-Y preparation at 1400-1500 ℃ by sol-gel method in Journal of Materials Research,1994,9(2):436-2Si2O7Document 4 "Trust P A, Chan K C, Ponton C B. Synthesis of synthetic single-phase microstructure specific derivative pre-heater using hydrothermally processing [ J]The preparation of beta-Y at 1300 ℃ by hydrothermal synthesis in Journal of Materials Research,1998,13(11):3135-3143 ″2Si2O7Reference 5 "Parmentier J, Philippie R.Bodart, Ludovic Audoin, et al.phase Transformations in Gel-Derived and Mixed-Powder-Derived Yttrium Disilacticate, Y2Si2O7,by X-Ray Diffraction and 29Si MAS NMR[J]16-20 of the Journal of Solid State Chemistry, 2000,149(1):16-20 ″, by sol-gel method at 1400-1600 deg.C2Si2O7And gamma-Y2Si2O7. Compared with the methods, the method solves the problem of damage to the fiber and the matrix caused by overhigh preparation temperature, and compared with the field-assisted sintering technology adopted in documents 1 and 2, the method adopts the field-assisted sintering technology at 1200 ℃ and Li+Preparation of beta-Y under catalysis2Si2O7Compared with the prior art, the method provided by the patent has lower cost. The method has the advantages of simple operation in the preparation process, strong repeatability, no influence on the shape of the material and industrial production. Provides a new method for preparing rare earth silicate ceramic and rare earth silicate modified ceramic matrix composite material by chemical vapor deposition.
Drawings
FIG. 1 is a nuclear magnetic resonance analysis chart of yttrium silicate crystal form prepared in embodiment 1 of the invention
FIG. 2 shows SiC modified with yttrium silicate prepared in examples 1 to 3 of the present inventionfPhase analysis diagram of/SiC composite material
FIG. 3 shows SiC modified with yttrium silicate prepared in example 3 of the present inventionfScanning photograph of/SiC composite material
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1
Step 1: preparing raw materials: 20 wt% of yttrium oxide, 75 wt% of water, 2 wt% of binder polyvinyl alcohol, 1 wt% of dispersant ammonium polyacrylate and 2 wt% of sintering aid lithium carbonate
Step 2: slurry preparation and impregnation:
a. magnetically stirring a solution obtained by mixing 75 wt% of water, 2 wt% of polyvinyl alcohol, 1 wt% of ammonium polyacrylate and 2 wt% of lithium carbonate for 30min at a stirring speed of 100 r/min;
b. adding wt 20% yttrium oxide into the obtained uniformly mixed liquid, and carrying out ball milling, wherein the rotating speed of a ball milling roller is 120r/min, and the ball milling time is 12h, so as to obtain uniformly mixed yttrium oxide slurry;
c. and (3) dipping the semi-compact ceramic matrix composite material into the yttrium oxide slurry in vacuum and pressure, and drying at 120 ℃.
And step 3: preparing yttrium silicate by chemical vapor deposition: with CH3SiCl3As precursor, CO2As oxygen source, hydrogen gas as carrier gas and diluent gas, argon gas as protective gas, gas flow rate ratio Q (H)2):Q(CH3SiCl3)＝9，Q(H2):Q(Ar)＝3，Q(H2):Q(CO2) 10:3, wherein the flow of argon is 120ml/min, the pressure in the furnace is kept at 2000Pa, the deposition temperature is 1100 ℃, the heat preservation time is 5h, and the yttrium silicate modified SiC is obtained by chemical vapor depositionfa/SiC composite material.
The yttrium silicate formed under the deposition conditions is X1-Y2SiO5And beta-Y2Si2O7The diffraction peak intensity was not high, indicating that the amount of yttrium silicate produced was small.
Example 2
Step 1: preparing raw materials: 20 wt% of yttrium oxide, 75 wt% of water, 2 wt% of binder polyvinyl alcohol, 1 wt% of dispersant ammonium polyacrylate and 2 wt% of sintering aid lithium carbonate
Step 2: slurry preparation and impregnation:
a. magnetically stirring a solution obtained by mixing 75 wt% of water, 2 wt% of polyvinyl alcohol, 1 wt% of ammonium polyacrylate and 2 wt% of lithium carbonate for 30min at a stirring speed of 100 r/min;
b. adding wt 20% yttrium oxide into the obtained uniformly mixed liquid, and carrying out ball milling, wherein the rotating speed of a ball milling roller is 120r/min, and the ball milling time is 12h, so as to obtain uniformly mixed yttrium oxide slurry;
c. and (3) dipping the semi-compact ceramic matrix composite material into the yttrium oxide slurry in vacuum and pressure, and drying at 120 ℃.
And step 3: preparing yttrium silicate by chemical vapor deposition: with CH3SiCl3As precursor, CO2As oxygen source, hydrogen gas as carrier gas and diluent gas, argon gas as protective gas, gas flow rate ratio Q (H)2):Q(CH3SiCl3)＝9，Q(H2):Q(Ar)＝3，Q(H2):Q(CO2) 10:3, wherein the flow of argon is 120ml/min, the pressure in the furnace is kept at 2000Pa, the deposition temperature is 1100 ℃, the heat preservation time is 10h, and the yttrium silicate modified SiC is obtained by chemical vapor depositionfa/SiC composite material.
Extension of the deposition time, Y2SiO5And Y2Si2O7The diffraction peak intensity is increased, the yield of the yttrium silicate is increased, and the further generation of the yttrium silicate is facilitated by prolonging the deposition time.
Example 3
Step 1: preparing raw materials: 20 wt% of yttrium oxide, 75 wt% of water, 2 wt% of binder polyvinyl alcohol, 1 wt% of dispersant ammonium polyacrylate and 2 wt% of sintering aid lithium carbonate
Step 2: slurry preparation and impregnation:
a. magnetically stirring a solution obtained by mixing 75 wt% of water, 2 wt% of polyvinyl alcohol, 1 wt% of ammonium polyacrylate and 2 wt% of lithium carbonate for 30min at a stirring speed of 100 r/min;
b. adding wt 20% yttrium oxide into the obtained uniformly mixed liquid, and carrying out ball milling, wherein the rotating speed of a ball milling roller is 120r/min, and the ball milling time is 12h, so as to obtain uniformly mixed yttrium oxide slurry;
c. and (3) dipping the semi-compact ceramic matrix composite material into the yttrium oxide slurry in vacuum and pressure, and drying at 120 ℃.
And step 3: preparing yttrium silicate by chemical vapor deposition: with CH3SiCl3As precursor, CO2As oxygen source, hydrogen gas as carrier gas and diluent gas, argon gas as protective gas, gas flow rate ratio Q (H)2):Q(CH3SiCl3)＝9，Q(H2):Q(Ar)＝3，Q(H2):Q(CO2) 10:3, wherein the flow of argon is 120ml/min, the pressure in the furnace is kept at 2000Pa, the deposition temperature is 1100 ℃, the heat preservation time is 15h, and the yttrium silicate modified SiC is obtained by chemical vapor depositionfa/SiC composite material.
The deposition time continues to increase, Y2Si2O7The strength is improved, the time is prolonged, and the crystal form of the yttrium silicate is transformed.
Example 4
Step 1: preparing raw materials: 15 wt% of ytterbium oxide, 80wt% of water, 2 wt% of binder polyvinyl alcohol, 1 wt% of dispersant ammonium polyacrylate and 2 wt% of sintering aid lithium carbonate
Step 2: slurry preparation and impregnation:
a. magnetically stirring a solution obtained by mixing 80wt% of water, 2 wt% of polyvinyl alcohol, 1 wt% of ammonium polyacrylate and 2 wt% of lithium carbonate for 30min at a stirring speed of 100 r/min;
b. adding 15 wt% ytterbium oxide into the obtained uniformly mixed liquid, and carrying out ball milling, wherein the rotating speed of a ball milling roller is 120r/min, and the ball milling time is 12h, so as to obtain uniformly mixed ytterbium oxide slurry;
c. and (3) dipping the semi-compact ceramic matrix composite material in vacuum and pressure with ytterbium oxide slurry, and drying at 120 ℃.
And step 3: preparing ytterbium silicate by chemical vapor deposition: with CH3SiCl3As precursor, CO2As oxygen source, hydrogen gas as carrier gas and diluent gas, argon gas as protective gas, gas flow rate ratio Q (H)2):Q(CH3SiCl3)＝9，Q(H2):Q(Ar)＝3，Q(H2):Q(CO2) 10:3, wherein the argon flow is 120ml/min, the pressure in the furnace is kept at 2000Pa, the deposition temperature is 1100 ℃,keeping the temperature for 15h, and obtaining the ytterbium silicate modified SiC by chemical vapor depositionfa/SiC composite material.
Example 5
Step 1: preparing raw materials: the material comprises, by weight, 15% of lutetium oxide, 80% of water, 2% of binder polyvinyl alcohol, 1% of dispersant ammonium polyacrylate and 2% of sintering aid lithium carbonate
Step 2: slurry preparation and impregnation:
a. magnetically stirring a solution obtained by mixing 80wt% of water, 2 wt% of polyvinyl alcohol, 1 wt% of ammonium polyacrylate and 2 wt% of lithium carbonate for 30min at a stirring speed of 100 r/min;
b. adding wt 15% lutetium oxide into the obtained uniformly mixed liquid, and carrying out ball milling, wherein the rotating speed of a ball milling roller is 120r/min, and the ball milling time is 12h, so as to obtain uniformly mixed lutetium oxide slurry;
c. and (3) dipping the semi-compact ceramic matrix composite material into lutetium oxide slurry in vacuum and pressure, and drying at 120 ℃.
And step 3: preparing lutetium silicate by chemical vapor deposition: with CH3SiCl3As precursor, CO2As oxygen source, hydrogen gas as carrier gas and diluent gas, argon gas as protective gas, gas flow rate ratio Q (H)2):Q(CH3SiCl3)＝9，Q(H2):Q(Ar)＝3，Q(H2):Q(CO2) 10:3, wherein the flow of argon is 120ml/min, the pressure in the furnace is kept at 2000Pa, the deposition temperature is 1100 ℃, the heat preservation time is 15h, and the lutetium silicate modified SiC is obtained by chemical vapor depositionfa/SiC composite material.

Claims (5)

1. A method for preparing rare earth silicate ceramic by adopting oxygen-containing precursor chemical vapor deposition is characterized by comprising the following steps:
step 1, preparing rare earth oxide slurry: magnetically stirring a solution obtained by mixing 70-80 wt% of water, 1-2 wt% of polyvinyl alcohol, 0.5-1 wt% of ammonium polyacrylate and 1-2 wt% of lithium carbonate;
adding 15-25 wt% of rare earth oxide, and performing ball milling to obtain uniformly mixed semi-compact ceramic matrix composite material impregnated rare earth oxide slurry;
the sum of the weight percentages of the components is 100 percent;
step 2, preparing rare earth silicate by chemical vapor deposition: vacuum and pressure dipping the semi-compact ceramic matrix composite material in rare earth oxide slurry at 120 deg.CoC, drying; with CH3SiCl3As precursor, CO2As oxygen source, hydrogen gas as carrier gas and diluent gas, argon gas as protective gas, gas flow rate ratio Q (H)2):Q(CH3SiCl3)＝6~9，Q(H2):Q(Ar)＝2~3，Q(H2):Q(CO2) = 2-4, wherein the flow rate of argon gas is 100-120 ml/min, the pressure in the furnace is kept at 2000Pa, and the deposition temperature is 1050-1200oAnd C, keeping the temperature for 5-15 h, and performing chemical vapor deposition to obtain the rare earth silicate ceramic.
2. The method for preparing rare earth silicate ceramics by oxygen-containing precursor chemical vapor deposition according to claim 1, wherein: the stirring time in the step 1 is 25-35 min, and the stirring speed is 100-120 r/min.
3. The method for preparing rare earth silicate ceramics by oxygen-containing precursor chemical vapor deposition according to claim 1, wherein: the rotating speed of the ball milling roller in the step 1 is 120-150 r/min, and the ball milling time is 10-15 h.
4. The method for preparing rare earth silicate ceramics by oxygen-containing precursor chemical vapor deposition according to claim 1, wherein: the rare earth oxide is yttrium oxide, ytterbium oxide, lutetium oxide and other rare earth oxides.
5. The method for preparing rare earth silicate ceramics by oxygen-containing precursor chemical vapor deposition according to claim 4, wherein: the particle size of the rare earth oxide is distributed between 0.1 and 20 microns.
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